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Hydrophobic catalyst, preparation method thereof and preparation method of beta-ionone

A technology of ionone and pseudoionone, applied in chemical instruments and methods, oxidation preparation of carbonyl compounds, physical/chemical process catalysts, etc., can solve problems such as low economic benefit, high cost of sulfuric acid wastewater treatment, and easy clogging

Active Publication Date: 2021-07-16
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can quickly remove the heat released by the reaction, the side reactions are greatly reduced, and the reaction process is easier to control, but the channel size of the microchannel reactor is small and easy to block, which is very inconvenient to use
[0005] Moreover, the existing production process of β-ionone usually adopts high-concentration sulfuric acid as the acid catalyst. After the reaction, a large amount of water is usually added to dilute the sulfuric acid, resulting in a large amount of waste water. The sulfuric acid produced in the production process of β-ionone Wastewater generally has low sulfuric acid concentration and high COD, and the treatment cost of sulfuric acid wastewater is high and the economic benefit is low.

Method used

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  • Hydrophobic catalyst, preparation method thereof and preparation method of beta-ionone
  • Hydrophobic catalyst, preparation method thereof and preparation method of beta-ionone
  • Hydrophobic catalyst, preparation method thereof and preparation method of beta-ionone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] To prepare the hydrophobic catalyst H-C1, proceed as follows:

[0079] (1) Dissolve N-methylpyrrole (40.56g, 0.5mol) in ether (162.23g), mix well and prepare solution a; dissolve trichloroacetyl chloride (186.37g, 1.03mol) in ether (1677.30 In g), mix evenly to prepare solution b; under nitrogen protection and stirring, at a reaction temperature of 40°C, add solution a dropwise to solution b for 7 hours, and continue to Stir the reaction for 4h, then quench the reaction with potassium carbonate aqueous solution (5wt%, 921.40g), separate the ether phase after standing, remove the ether in vacuum, recrystallize with isopropanol, and obtain a solid after vacuum drying Its nuclear magnetic analysis data are: 1 H NMR (400MHz, CDCl 3 ,298K)δ=7.50(2H,s, Ar- H ),3.59(3H,s,N CH 3 ).

[0080] (2) Will (74.37g, 0.2mol) was dissolved in N, N-dimethylformamide (855.23g), mixed uniformly and prepared into solution c; triethylenetetramine (30.71g, 0.21mol) was dissolved in ...

Embodiment 2

[0083] To prepare the hydrophobic catalyst H-C2, proceed as follows:

[0084] (1) Dissolve N-methylpyrrole (40.56g, 0.5mol) in ether (60.84g), mix well and prepare solution a; dissolve trichloroacetyl chloride (272.73g, 1.50mol) in ether (636.37 In g), mix evenly to prepare solution b; under nitrogen protection and stirring, at a reaction temperature of 80°C, add solution a dropwise to solution b for 3 hours, and continue to Stir the reaction for 2h, then quench the reaction with potassium carbonate aqueous solution (20wt%, 138.21g), separate the ether phase after standing, remove the ether in vacuum, recrystallize with isopropanol, and obtain a solid after vacuum drying

[0085] (2) Will (74.37g, 0.2mol) was dissolved in N, N-dimethylformamide (338.79g), mixed uniformly and prepared into solution c; triethylenetetramine (35.10g, 0.24mol) was dissolved in N, N - Dimethylformamide (184.26g), mixed evenly to prepare solution d; under nitrogen protection and stirring, at a r...

Embodiment 3

[0088] Prepare hydrophobic catalyst H-C3, carry out according to the following steps:

[0089] (1) Dissolve N-ethylpyrrole (47.57g, 0.5mol) in ether (111.00g), mix well and prepare solution a; dissolve trichloroacetyl chloride (227.28g, 1.25mol) in ether (909.11 In g), mix uniformly to prepare solution b; under nitrogen protection and stirring, at a reaction temperature of 60°C, add solution a dropwise to solution b for 5 hours, and continue to Stir the reaction for 3h, then quench the reaction with potassium carbonate aqueous solution (12.5wt%, 276.42g), separate the ether phase after standing, remove the ether in vacuum, recrystallize with isopropanol, and obtain a solid after vacuum drying

[0090] (2) Will (77.17g, 0.2mol) was dissolved in N, N-dimethylformamide (516.47g), mixed uniformly and prepared into solution c; triethylenetetramine (33.05g, 0.23mol) was dissolved in N, N -Dimethylformamide (221.18g), mixed evenly to prepare solution d; under nitrogen protection...

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PUM

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Abstract

The invention relates to a hydrophobic catalyst and a preparation method thereof, and a preparation method of beta-ionone, the hydrophobic catalyst prepared by the method can catalyze pseudoionone to form an intermediate, and then indirect acid catalysis reaction is performed to prepare the beta-ionone. The method has the characteristics of low requirements on equipment, mild operation conditions and no generation of sulfuric acid wastewater, and the yield of beta-ionone is high.

Description

technical field [0001] The invention relates to the field of preparation and catalyst of β-ionone, in particular to a hydrophobic catalyst, a preparation method thereof and a method for preparing β-ionone by using the catalyst. Background technique [0002] β-ionone [4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one, β-ionone] is a kind of precious spice, which also has certain Biological activity, showing a strong anti-cancer effect, especially the obvious inhibitory effect on the occurrence of tumors. In addition, this product is widely used in industry and is a very important pharmaceutical intermediate and an important raw material for the synthesis of vitamins A, E, β-carotene, carotenoids, retinoic acid and phytol. [0003] The synthesis of β-ionone is generally generated by direct cyclization reaction of pseudoionone as raw material under acid catalysis. The product of direct acid-catalyzed reaction is usually a mixture of isomers such as α-ionone, β-ionone and γ-ion...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C49/21C07C45/29
CPCB01J31/2213B01J31/1805C07C45/29B01J2531/22B01J2531/23B01J2531/24B01J2531/25C07C49/21
Inventor 林龙李金明张涛吕英东黎源张弈宇罗朝辉张旭郭劲资程晓波王延斌翟文超
Owner WANHUA CHEM GRP CO LTD
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